Biphasic calcium phosphate powders (BCP) of hydroxyapatite (HA) and tricalcium phosphate (β-TCP) with the various ratio of HA to β-TCP were prepared by utilizing mechanochemical synthesis. Calcium hydrogen-phosphate dihydrate (brushite, CaHPO4⋅2H2O) and calcium carbonate (calcite, CaCO3) powders have been chosen as the starting materials. The original Ca/P ratio of CaHPO4⋅2H2O - CaCO3 batch was set to be 1.67. A mixture of starting materials was milled using a planetary mill (ZrO2 jar and balls) with water for 3, 4, 5, 6 and 7 hrs. The XRD study of calcined powders was conducted for phase identification and for HA/β-TCP ratio as well. The phases of the calcined powders were HA and β-TCP, and the HA/β-TCP ratio varied with the milling time. The mass fraction of HA and β-TCP phases was calculated from the XRD intensities of HA and β-TCP. The ratio of the mixture milled for 4 hrs and calcined at 900°C was 85(HA):15(β-TCP) (BCP 85/15) and the content of β-TCP increased with the milling time. It is believed defective HA powder formed at relatively short period of milling time (less than 3 hrs The research revealed that nanocrystalline BCP powders could be synthesized by an employment of a medium-high energy mechanical activation at room temperatures (~25°C) without any preliminary chemical processing.